# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_20140623b_0m
_database_code_depnum_ccdc_archive 'CCDC 1020987'
_audit_update_record             
;
2014-08-25 deposited with the CCDC.
2014-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 B Cl2 F2 N3 O S'
_chemical_formula_weight         518.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.5908(8)
_cell_length_b                   10.9141(10)
_cell_length_c                   22.863(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.059(2)
_cell_angle_gamma                90.00
_cell_volume                     2363.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2844
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      24.10

_exptl_crystal_description       culumn
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8766
_exptl_absorpt_correction_T_max  0.8929
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12752
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.20
_reflns_number_total             4225
_reflns_number_gt                3073
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0766P)²+1.2456P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4225
_refine_ls_number_parameters     335
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1529
_refine_ls_wR_factor_gt          0.1299
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.7500(3) 0.6283(3) 0.02879(14) 0.0404(8) Uani 1 1 d . . .
C1 C 0.4559(8) 0.1621(9) 0.2076(4) 0.110(3) Uani 0.691(10) 1 d PU A 1
H1A H 0.4277 0.1042 0.2351 0.165 Uiso 0.691(10) 1 d PR A 1
H1B H 0.4258 0.1337 0.1679 0.165 Uiso 0.691(10) 1 d PR A 1
H1C H 0.4132 0.2401 0.2128 0.165 Uiso 0.691(10) 1 d PR A 1
C2 C 0.6851(10) 0.0547(6) 0.2150(4) 0.097(3) Uani 0.691(10) 1 d PU A 1
H2A H 0.7860 0.0628 0.2220 0.145 Uiso 0.691(10) 1 d PR A 1
H2B H 0.6553 0.0219 0.1761 0.145 Uiso 0.691(10) 1 d PR A 1
H2C H 0.6564 0.0005 0.2439 0.145 Uiso 0.691(10) 1 d PR A 1
C3 C 0.6586(11) 0.2246(7) 0.2828(3) 0.095(3) Uani 0.691(10) 1 d PU A 1
H3A H 0.6171 0.3039 0.2857 0.142 Uiso 0.691(10) 1 d PR A 1
H3B H 0.7595 0.2310 0.2922 0.142 Uiso 0.691(10) 1 d PR A 1
H3C H 0.6247 0.1694 0.3100 0.142 Uiso 0.691(10) 1 d PR A 1
C1' C 0.5246(19) 0.0862(15) 0.1841(6) 0.083(5) Uani 0.309(10) 1 d PU A 2
H1D H 0.4981 0.0234 0.2096 0.125 Uiso 0.309(10) 1 d PR A 2
H1E H 0.5712 0.0497 0.1543 0.125 Uiso 0.309(10) 1 d PR A 2
H1F H 0.4417 0.1288 0.1656 0.125 Uiso 0.309(10) 1 d PR A 2
C2' C 0.7464(17) 0.1008(18) 0.2540(9) 0.100(6) Uani 0.309(10) 1 d PU A 2
H2D H 0.7953 0.1502 0.2855 0.150 Uiso 0.309(10) 1 d PR A 2
H2E H 0.8102 0.0786 0.2273 0.150 Uiso 0.309(10) 1 d PR A 2
H2F H 0.7115 0.0279 0.2703 0.150 Uiso 0.309(10) 1 d PR A 2
C3' C 0.548(2) 0.2415(15) 0.2635(7) 0.084(5) Uani 0.309(10) 1 d PU A 2
H3D H 0.4777 0.2971 0.2441 0.126 Uiso 0.309(10) 1 d PR A 2
H3E H 0.6176 0.2864 0.2897 0.126 Uiso 0.309(10) 1 d PR A 2
H3F H 0.5035 0.1826 0.2858 0.126 Uiso 0.309(10) 1 d PR A 2
C4 C 0.6190(3) 0.1764(3) 0.21936(13) 0.0504(8) Uani 1 1 d . . .
C5 C 0.6711(3) 0.2692(3) 0.17768(11) 0.0425(7) Uani 1 1 d . A .
C6 C 0.8148(3) 0.2863(3) 0.17800(11) 0.0413(7) Uani 1 1 d . . .
H6 H 0.8802 0.2388 0.2025 0.050 Uiso 1 1 calc R A .
C7 C 0.8601(3) 0.3743(3) 0.14179(11) 0.0363(6) Uani 1 1 d . A .
C8 C 0.7643(3) 0.4473(3) 0.10464(11) 0.0353(6) Uani 1 1 d . . .
C9 C 0.6208(3) 0.4281(3) 0.10245(12) 0.0438(7) Uani 1 1 d . A .
H9 H 0.5552 0.4734 0.0769 0.053 Uiso 1 1 calc R . .
C10 C 0.5777(3) 0.3405(3) 0.13899(12) 0.0460(7) Uani 1 1 d . . .
H10 H 0.4814 0.3283 0.1378 0.055 Uiso 1 1 calc R A .
C11 C 0.9698(3) 0.5272(3) 0.08389(11) 0.0352(6) Uani 1 1 d . . .
C12 C 1.0093(3) 0.6856(2) 0.02267(10) 0.0334(6) Uani 1 1 d . . .
C13 C 1.1133(3) 0.7621(3) -0.00077(11) 0.0362(6) Uani 1 1 d . A .
C14 C 1.0659(3) 0.8615(3) -0.03853(11) 0.0371(6) Uani 1 1 d . . .
C15 C 0.9208(3) 0.8823(3) -0.05623(11) 0.0382(6) Uani 1 1 d . A .
C16 C 0.8174(3) 0.8008(3) -0.03451(11) 0.0401(7) Uani 1 1 d . . .
C17 C 0.8752(3) 0.9782(3) -0.09324(12) 0.0458(7) Uani 1 1 d . . .
H17 H 0.7791 0.9907 -0.1053 0.055 Uiso 1 1 calc R A .
C18 C 0.9731(4) 1.0572(3) -0.11287(13) 0.0518(8) Uani 1 1 d . A .
H18 H 0.9417 1.1223 -0.1377 0.062 Uiso 1 1 calc R . .
C19 C 1.1146(4) 1.0390(3) -0.09567(13) 0.0512(8) Uani 1 1 d . . .
H19 H 1.1784 1.0928 -0.1087 0.061 Uiso 1 1 calc R A .
C20 C 1.1656(3) 0.9409(3) -0.05879(12) 0.0428(7) Uani 1 1 d . A .
C21 C 1.3108(3) 0.9172(3) -0.04054(13) 0.0529(8) Uani 1 1 d . . .
H21 H 1.3775 0.9694 -0.0525 0.063 Uiso 1 1 calc R A .
C22 C 1.3541(3) 0.8201(3) -0.00604(14) 0.0532(8) Uani 1 1 d . A .
H22 H 1.4502 0.8051 0.0045 0.064 Uiso 1 1 calc R . .
C23 C 0.1375(6) 0.1380(6) 0.3252(2) 0.124(2) Uani 1 1 d . . .
H23A H 0.2273 0.1212 0.3499 0.149 Uiso 1 1 calc R . .
H23B H 0.0636 0.1098 0.3464 0.149 Uiso 1 1 calc R . .
C24 C 1.2562(3) 0.7411(3) 0.01436(13) 0.0462(7) Uani 1 1 d . . .
H24 H 1.2880 0.6745 0.0381 0.055 Uiso 1 1 calc R A .
Cl1 Cl 0.1210(2) 0.29232(18) 0.31573(11) 0.1831(10) Uani 1 1 d . . .
Cl2 Cl 0.12870(17) 0.05639(19) 0.26224(8) 0.1411(7) Uani 1 1 d . . .
F1 F 0.67166(17) 0.70163(17) 0.06058(8) 0.0587(5) Uani 1 1 d . . .
F2 F 0.66850(17) 0.56722(18) -0.01626(8) 0.0593(5) Uani 1 1 d . . .
N1 N 0.8297(2) 0.5331(2) 0.07229(9) 0.0347(5) Uani 1 1 d . A .
N2 N 1.0602(2) 0.6000(2) 0.06092(9) 0.0377(5) Uani 1 1 d . A .
N3 N 0.8686(2) 0.7065(2) 0.00543(9) 0.0344(5) Uani 1 1 d . A .
O1 O 0.6908(2) 0.8146(2) -0.04865(10) 0.0594(6) Uani 1 1 d . A .
S1 S 1.03275(7) 0.41602(7) 0.13513(3) 0.0415(2) Uani 1 1 d . A .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 F2 1.364(4) . ?
B1 F1 1.380(4) . ?
B1 N1 1.554(4) . ?
B1 N3 1.581(4) . ?
C1 C4 1.553(7) . ?
C2 C4 1.481(7) . ?
C3 C4 1.533(7) . ?
C1' C4 1.486(13) . ?
C2' C4 1.580(16) . ?
C3' C4 1.486(14) . ?
C4 C5 1.528(4) . ?
C5 C6 1.390(4) . ?
C5 C10 1.393(4) . ?
C6 C7 1.382(4) . ?
C7 C8 1.397(4) . ?
C7 S1 1.747(3) . ?
C8 C9 1.385(4) . ?
C8 N1 1.401(3) . ?
C9 C10 1.375(4) . ?
C11 N1 1.329(3) . ?
C11 N2 1.343(3) . ?
C11 S1 1.728(3) . ?
C12 N2 1.319(3) . ?
C12 N3 1.365(3) . ?
C12 C13 1.464(4) . ?
C13 C24 1.379(4) . ?
C13 C14 1.416(4) . ?
C14 C15 1.405(4) . ?
C14 C20 1.421(4) . ?
C15 C17 1.373(4) . ?
C15 C16 1.475(4) . ?
C16 O1 1.216(3) . ?
C16 N3 1.411(3) . ?
C17 C18 1.400(4) . ?
C18 C19 1.367(4) . ?
C19 C20 1.402(4) . ?
C20 C21 1.413(4) . ?
C21 C22 1.347(5) . ?
C22 C24 1.407(4) . ?
C23 Cl2 1.684(6) . ?
C23 Cl1 1.702(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 B1 F1 112.7(2) . . ?
F2 B1 N1 108.8(2) . . ?
F1 B1 N1 107.7(2) . . ?
F2 B1 N3 111.4(2) . . ?
F1 B1 N3 110.2(3) . . ?
N1 B1 N3 105.6(2) . . ?
C2 C4 C3' 136.2(7) . . ?
C2 C4 C1' 66.4(8) . . ?
C3' C4 C1' 112.2(10) . . ?
C2 C4 C5 111.6(3) . . ?
C3' C4 C5 109.7(6) . . ?
C1' C4 C5 109.4(5) . . ?
C2 C4 C3 109.0(5) . . ?
C3' C4 C3 42.8(7) . . ?
C1' C4 C3 141.2(6) . . ?
C5 C4 C3 107.8(3) . . ?
C2 C4 C1 109.2(5) . . ?
C3' C4 C1 66.8(8) . . ?
C1' C4 C1 47.8(7) . . ?
C5 C4 C1 112.2(3) . . ?
C3 C4 C1 106.9(5) . . ?
C2 C4 C2' 42.3(8) . . ?
C3' C4 C2' 108.2(10) . . ?
C1' C4 C2' 106.4(10) . . ?
C5 C4 C2' 110.9(6) . . ?
C3 C4 C2' 69.4(9) . . ?
C1 C4 C2' 135.5(6) . . ?
C6 C5 C10 117.8(3) . . ?
C6 C5 C4 120.5(3) . . ?
C10 C5 C4 121.7(3) . . ?
C7 C6 C5 119.7(3) . . ?
C6 C7 C8 121.4(2) . . ?
C6 C7 S1 128.7(2) . . ?
C8 C7 S1 109.9(2) . . ?
C9 C8 C7 119.3(2) . . ?
C9 C8 N1 127.3(2) . . ?
C7 C8 N1 113.3(2) . . ?
C10 C9 C8 118.3(3) . . ?
C9 C10 C5 123.3(3) . . ?
N1 C11 N2 126.0(2) . . ?
N1 C11 S1 113.80(19) . . ?
N2 C11 S1 120.18(19) . . ?
N2 C12 N3 123.7(2) . . ?
N2 C12 C13 116.4(2) . . ?
N3 C12 C13 119.9(2) . . ?
C24 C13 C14 119.4(3) . . ?
C24 C13 C12 121.4(3) . . ?
C14 C13 C12 119.2(2) . . ?
C15 C14 C13 120.5(2) . . ?
C15 C14 C20 119.6(3) . . ?
C13 C14 C20 119.9(3) . . ?
C17 C15 C14 120.3(3) . . ?
C17 C15 C16 120.1(3) . . ?
C14 C15 C16 119.6(2) . . ?
O1 C16 N3 119.6(3) . . ?
O1 C16 C15 122.1(3) . . ?
N3 C16 C15 118.3(2) . . ?
C15 C17 C18 120.2(3) . . ?
C19 C18 C17 120.3(3) . . ?
C18 C19 C20 121.4(3) . . ?
C19 C20 C21 123.5(3) . . ?
C19 C20 C14 118.2(3) . . ?
C21 C20 C14 118.3(3) . . ?
C22 C21 C20 121.1(3) . . ?
C21 C22 C24 121.0(3) . . ?
Cl2 C23 Cl1 115.1(4) . . ?
C13 C24 C22 120.3(3) . . ?
C11 N1 C8 112.6(2) . . ?
C11 N1 B1 122.7(2) . . ?
C8 N1 B1 124.7(2) . . ?
C12 N2 C11 119.0(2) . . ?
C12 N3 C16 122.4(2) . . ?
C12 N3 B1 123.0(2) . . ?
C16 N3 B1 114.6(2) . . ?
C11 S1 C7 90.41(12) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.053
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cu_20140704a_0m
_database_code_depnum_ccdc_archive 'CCDC 1020988'
_audit_update_record             
;
2014-08-25 deposited with the CCDC.
2014-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H26 B F2 N3 O2 S'
_chemical_formula_weight         505.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.57220(10)
_cell_length_b                   16.04600(10)
_cell_length_c                   22.1206(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.66
_cell_angle_gamma                90.00
_cell_volume                     4928.66(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       culumn
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112
_exptl_absorpt_coefficient_mu    1.555
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_T_max  0.8600
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24376
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.21
_diffrn_reflns_theta_max         68.16
_reflns_number_total             8642
_reflns_number_gt                7368
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1359P)²+2.4185P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8642
_refine_ls_number_parameters     649
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.2339
_refine_ls_wR_factor_gt          0.2230
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.9890(2) 0.5182(2) 0.15519(18) 0.0577(8) Uani 1 1 d . . .
B2 B 0.4836(2) 0.5386(2) 0.15811(17) 0.0555(7) Uani 1 1 d . . .
C1 C 1.1415(2) 0.60142(18) 0.20195(14) 0.0568(7) Uani 1 1 d . . .
C2 C 1.1940(2) 0.67960(18) 0.22480(13) 0.0552(7) Uani 1 1 d . . .
C3 C 1.2918(2) 0.6783(2) 0.25285(16) 0.0676(8) Uani 1 1 d . . .
H3 H 1.3250 0.6281 0.2573 0.081 Uiso 1 1 calc R . .
C4 C 1.3420(3) 0.7522(2) 0.27490(18) 0.0763(9) Uani 1 1 d . . .
H4 H 1.4082 0.7506 0.2941 0.092 Uiso 1 1 calc R . .
C5 C 1.2943(3) 0.8269(2) 0.26849(17) 0.0723(9) Uani 1 1 d . . .
H5 H 1.3282 0.8754 0.2839 0.087 Uiso 1 1 calc R . .
C6 C 1.1939(2) 0.83057(19) 0.23870(15) 0.0615(7) Uani 1 1 d . . .
C7 C 1.1410(3) 0.9057(2) 0.22912(16) 0.0693(8) Uani 1 1 d . . .
H7 H 1.1726 0.9556 0.2435 0.083 Uiso 1 1 calc R . .
C8 C 1.0448(3) 0.90650(19) 0.19933(17) 0.0700(8) Uani 1 1 d . . .
H8 H 1.0116 0.9568 0.1936 0.084 Uiso 1 1 calc R . .
C9 C 0.9950(2) 0.83264(18) 0.17714(15) 0.0615(7) Uani 1 1 d . . .
H9 H 0.9291 0.8342 0.1565 0.074 Uiso 1 1 calc R . .
C10 C 1.1435(2) 0.75536(18) 0.21648(13) 0.0528(6) Uani 1 1 d . . .
C11 C 1.0435(2) 0.75717(17) 0.18588(13) 0.0527(6) Uani 1 1 d . . .
C12 C 0.9918(2) 0.67930(17) 0.16530(13) 0.0520(6) Uani 1 1 d . . .
C13 C 0.8466(2) 0.61533(17) 0.12093(14) 0.0550(7) Uani 1 1 d . . .
C14 C 0.7166(2) 0.51497(19) 0.07974(14) 0.0576(7) Uani 1 1 d . . .
C15 C 0.8077(2) 0.47875(18) 0.10307(13) 0.0537(6) Uani 1 1 d . . .
C16 C 0.8178(2) 0.39315(18) 0.10179(14) 0.0582(7) Uani 1 1 d . . .
H16 H 0.8782 0.3686 0.1177 0.070 Uiso 1 1 calc R . .
C17 C 0.7364(2) 0.3445(2) 0.07643(14) 0.0608(7) Uani 1 1 d . . .
H17 H 0.7424 0.2869 0.0750 0.073 Uiso 1 1 calc R . .
C18 C 0.6351(2) 0.4668(2) 0.05451(15) 0.0646(8) Uani 1 1 d . . .
H18 H 0.5748 0.4915 0.0390 0.078 Uiso 1 1 calc R . .
C19 C 0.6453(2) 0.3815(2) 0.05285(15) 0.0619(7) Uani 1 1 d . . .
C20 C 0.5638(3) 0.2512(2) 0.02250(18) 0.0743(9) Uani 1 1 d . . .
H20A H 0.5856 0.2255 0.0641 0.089 Uiso 1 1 calc R . .
H20B H 0.6068 0.2348 -0.0013 0.089 Uiso 1 1 calc R . .
C21 C 0.4617(3) 0.2255(3) -0.0120(2) 0.0837(10) Uani 1 1 d . . .
H21A H 0.4194 0.2482 0.0103 0.100 Uiso 1 1 calc R . .
H21B H 0.4431 0.2497 -0.0542 0.100 Uiso 1 1 calc R . .
C22 C 0.4475(3) 0.1342(3) -0.0178(2) 0.0864(11) Uani 1 1 d . . .
H22A H 0.4598 0.1106 0.0243 0.104 Uiso 1 1 calc R . .
H22B H 0.4942 0.1107 -0.0363 0.104 Uiso 1 1 calc R . .
C23 C 0.3451(3) 0.1086(3) -0.0589(2) 0.0867(11) Uani 1 1 d . . .
H23A H 0.2984 0.1325 -0.0406 0.104 Uiso 1 1 calc R . .
H23B H 0.3331 0.1319 -0.1011 0.104 Uiso 1 1 calc R . .
C24 C 0.3303(3) 0.0171(3) -0.0644(2) 0.0936(12) Uani 1 1 d . . .
H24A H 0.3466 -0.0066 -0.0221 0.112 Uiso 1 1 calc R . .
H24B H 0.3740 -0.0063 -0.0854 0.112 Uiso 1 1 calc R . .
C25 C 0.2285(3) -0.0077(3) -0.10079(19) 0.0866(11) Uani 1 1 d . . .
H25A H 0.2144 0.0108 -0.1444 0.104 Uiso 1 1 calc R . .
H25B H 0.1841 0.0203 -0.0825 0.104 Uiso 1 1 calc R . .
C26 C 0.2122(3) -0.1010(3) -0.1001(2) 0.0943(12) Uani 1 1 d . . .
H26A H 0.2562 -0.1285 -0.1189 0.113 Uiso 1 1 calc R . .
H26B H 0.2281 -0.1193 -0.0563 0.113 Uiso 1 1 calc R . .
C27 C 0.1124(4) -0.1282(3) -0.1343(3) 0.1097(15) Uani 1 1 d . . .
H27A H 0.0683 -0.1035 -0.1149 0.164 Uiso 1 1 d R . .
H27B H 0.1087 -0.1878 -0.1322 0.164 Uiso 1 1 d R . .
H27C H 0.0959 -0.1111 -0.1779 0.164 Uiso 1 1 d R . .
C28 C 0.6343(2) 0.45499(17) 0.20598(14) 0.0549(7) Uani 1 1 d . . .
C29 C 0.6882(2) 0.37604(17) 0.22263(13) 0.0546(7) Uani 1 1 d . . .
C30 C 0.7857(2) 0.3771(2) 0.25112(16) 0.0667(8) Uani 1 1 d . . .
H30 H 0.8184 0.4277 0.2589 0.080 Uiso 1 1 calc R . .
C31 C 0.8365(3) 0.3025(2) 0.26859(19) 0.0778(10) Uani 1 1 d . . .
H31 H 0.9028 0.3038 0.2877 0.093 Uiso 1 1 calc R . .
C32 C 0.7894(3) 0.2274(2) 0.25787(17) 0.0727(9) Uani 1 1 d . . .
H32 H 0.8238 0.1784 0.2705 0.087 Uiso 1 1 calc R . .
C33 C 0.6896(2) 0.22407(19) 0.22802(14) 0.0612(7) Uani 1 1 d . . .
C34 C 0.6380(3) 0.1488(2) 0.21653(17) 0.0705(9) Uani 1 1 d . . .
H34 H 0.6701 0.0987 0.2292 0.085 Uiso 1 1 calc R . .
C35 C 0.5409(3) 0.1485(2) 0.18694(18) 0.0752(9) Uani 1 1 d . . .
H35 H 0.5077 0.0982 0.1801 0.090 Uiso 1 1 calc R . .
C36 C 0.4906(3) 0.22303(19) 0.16678(16) 0.0651(8) Uani 1 1 d . . .
H36 H 0.4247 0.2217 0.1461 0.078 Uiso 1 1 calc R . .
C37 C 0.5388(2) 0.29829(17) 0.17768(13) 0.0545(7) Uani 1 1 d . . .
C38 C 0.6384(2) 0.29966(17) 0.20935(13) 0.0536(6) Uani 1 1 d . . .
C39 C 0.4871(2) 0.37747(17) 0.15775(14) 0.0534(6) Uani 1 1 d . . .
C40 C 0.3440(2) 0.44206(18) 0.10872(15) 0.0572(7) Uani 1 1 d . . .
C41 C 0.2159(2) 0.5445(2) 0.06734(14) 0.0592(7) Uani 1 1 d . . .
C42 C 0.3056(2) 0.57953(18) 0.09702(14) 0.0553(7) Uani 1 1 d . . .
C43 C 0.3156(2) 0.66563(19) 0.10147(15) 0.0617(7) Uani 1 1 d . . .
H43 H 0.3753 0.6899 0.1208 0.074 Uiso 1 1 calc R . .
C44 C 0.2353(2) 0.7138(2) 0.07668(16) 0.0705(8) Uani 1 1 d . . .
H44 H 0.2409 0.7715 0.0795 0.085 Uiso 1 1 calc R . .
C45 C 0.1443(3) 0.6782(2) 0.04701(16) 0.0720(9) Uani 1 1 d . . .
C46 C 0.1340(2) 0.5930(2) 0.04138(16) 0.0674(8) Uani 1 1 d . . .
H46 H 0.0747 0.5687 0.0210 0.081 Uiso 1 1 calc R . .
C47 C -0.0219(4) 0.7039(4) -0.0052(3) 0.1201(17) Uani 1 1 d DU . .
H47A H -0.0369 0.6575 0.0183 0.144 Uiso 1 1 calc R . .
H47B H -0.0257 0.6846 -0.0474 0.144 Uiso 1 1 calc R . .
C48 C -0.0930(5) 0.7734(5) -0.0094(4) 0.179(3) Uani 1 1 d DU . .
H48A H -0.1580 0.7517 -0.0257 0.215 Uiso 1 1 calc R . .
H48B H -0.0849 0.7958 0.0326 0.215 Uiso 1 1 calc R . .
C49 C -0.0801(6) 0.8349(6) -0.0480(4) 0.178(3) Uani 1 1 d DU . .
H49A H -0.0845 0.8132 -0.0897 0.214 Uiso 1 1 calc R . .
H49B H -0.0176 0.8611 -0.0303 0.214 Uiso 1 1 calc R . .
C50 C -0.1632(8) 0.8986(7) -0.0519(5) 0.234(5) Uani 1 1 d DU . .
H50A H -0.2240 0.8689 -0.0657 0.281 Uiso 1 1 calc R . .
H50B H -0.1557 0.9196 -0.0095 0.281 Uiso 1 1 calc R . .
C51 C -0.1686(8) 0.9662(6) -0.0919(4) 0.219(4) Uani 1 1 d DU . .
H51A H -0.1794 0.9435 -0.1341 0.263 Uiso 1 1 calc R . .
H51B H -0.1050 0.9911 -0.0797 0.263 Uiso 1 1 calc R . .
C52 C -0.2395(6) 1.0374(4) -0.0986(3) 0.147(2) Uani 1 1 d U . .
H52A H -0.2335 1.0583 -0.0564 0.176 Uiso 1 1 calc R . .
H52B H -0.2197 1.0820 -0.1216 0.176 Uiso 1 1 calc R . .
C53 C -0.3354(6) 1.0216(5) -0.1283(3) 0.149(2) Uani 1 1 d U . .
H53A H -0.3568 0.9810 -0.1030 0.178 Uiso 1 1 calc R . .
H53B H -0.3408 0.9956 -0.1689 0.178 Uiso 1 1 calc R . .
C54 C -0.4054(4) 1.0956(4) -0.1405(2) 0.1166(16) Uani 1 1 d U . .
H54A H -0.4047 1.1195 -0.1006 0.175 Uiso 1 1 d R . .
H54B H -0.4694 1.0771 -0.1628 0.175 Uiso 1 1 d R . .
H54C H -0.3854 1.1367 -0.1655 0.175 Uiso 1 1 d R . .
F1 F 1.02014(13) 0.47821(12) 0.10995(11) 0.0807(6) Uani 1 1 d . . .
F2 F 1.00100(15) 0.46920(12) 0.20803(11) 0.0857(6) Uani 1 1 d . . .
F3 F 0.52249(13) 0.58764(11) 0.12134(10) 0.0723(5) Uani 1 1 d . . .
F4 F 0.48412(14) 0.57924(11) 0.21347(9) 0.0743(5) Uani 1 1 d . . .
N1 N 1.04110(17) 0.60465(14) 0.17403(11) 0.0522(5) Uani 1 1 d . . .
N2 N 0.89824(17) 0.68520(15) 0.13857(12) 0.0571(6) Uani 1 1 d . . .
N3 N 0.88048(17) 0.53783(14) 0.12615(11) 0.0533(5) Uani 1 1 d . . .
N4 N 0.53544(17) 0.45167(14) 0.17317(11) 0.0520(5) Uani 1 1 d . . .
N5 N 0.39540(18) 0.37187(14) 0.12585(13) 0.0588(6) Uani 1 1 d . . .
N6 N 0.37708(17) 0.51948(14) 0.12014(11) 0.0541(6) Uani 1 1 d . . .
O1 O 0.56179(16) 0.33914(16) 0.02802(12) 0.0774(7) Uani 1 1 d . . .
O2 O 1.18240(16) 0.53456(14) 0.20693(12) 0.0754(7) Uani 1 1 d . . .
O3 O 0.67325(16) 0.52246(13) 0.22007(12) 0.0725(6) Uani 1 1 d . . .
O4 O 0.0708(2) 0.7331(2) 0.02549(16) 0.1067(10) Uani 1 1 d . . .
S1 S 0.72378(6) 0.62231(5) 0.08814(4) 0.0671(3) Uani 1 1 d . . .
S2 S 0.22271(6) 0.43666(5) 0.06910(4) 0.0684(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 F2 1.376(4) . ?
B1 F1 1.377(4) . ?
B1 N3 1.548(4) . ?
B1 N1 1.575(4) . ?
B2 F3 1.372(4) . ?
B2 F4 1.385(4) . ?
B2 N6 1.555(4) . ?
B2 N4 1.574(4) . ?
C1 O2 1.216(4) . ?
C1 N1 1.405(4) . ?
C1 C2 1.477(4) . ?
C2 C3 1.370(4) . ?
C2 C10 1.404(4) . ?
C3 C4 1.401(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.413(5) . ?
C6 C10 1.421(4) . ?
C7 C8 1.355(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(4) . ?
C8 H8 0.9300 . ?
C9 C11 1.386(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.409(4) . ?
C11 C12 1.459(4) . ?
C12 N2 1.315(4) . ?
C12 N1 1.380(3) . ?
C13 N3 1.330(4) . ?
C13 N2 1.341(4) . ?
C13 S1 1.719(3) . ?
C14 C18 1.385(4) . ?
C14 C15 1.397(4) . ?
C14 S1 1.732(3) . ?
C15 C16 1.383(4) . ?
C15 N3 1.398(4) . ?
C16 C17 1.388(4) . ?
C16 H16 0.9300 . ?
C17 C19 1.403(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(5) . ?
C18 H18 0.9300 . ?
C19 O1 1.356(4) . ?
C20 O1 1.417(4) . ?
C20 C21 1.509(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.480(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.550(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.483(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.511(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.517(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.487(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 O3 1.218(3) . ?
C28 N4 1.404(4) . ?
C28 C29 1.477(4) . ?
C29 C30 1.368(4) . ?
C29 C38 1.409(4) . ?
C30 C31 1.399(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.370(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.403(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.405(5) . ?
C33 C38 1.418(4) . ?
C34 C35 1.366(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.403(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.381(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.408(4) . ?
C37 C39 1.475(4) . ?
C39 N5 1.311(4) . ?
C39 N4 1.373(3) . ?
C40 N6 1.329(4) . ?
C40 N5 1.342(4) . ?
C40 S2 1.721(3) . ?
C41 C42 1.391(4) . ?
C41 C46 1.394(5) . ?
C41 S2 1.732(3) . ?
C42 C43 1.390(4) . ?
C42 N6 1.397(4) . ?
C43 C44 1.371(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.409(5) . ?
C44 H44 0.9300 . ?
C45 O4 1.356(4) . ?
C45 C46 1.378(5) . ?
C46 H46 0.9300 . ?
C47 O4 1.396(6) . ?
C47 C48 1.505(7) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.355(7) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C50 1.567(8) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C51 1.386(8) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.517(9) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.376(9) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.535(8) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 B1 F1 111.4(3) . . ?
F2 B1 N3 108.6(3) . . ?
F1 B1 N3 108.3(3) . . ?
F2 B1 N1 110.6(3) . . ?
F1 B1 N1 111.4(3) . . ?
N3 B1 N1 106.3(2) . . ?
F3 B2 F4 111.2(3) . . ?
F3 B2 N6 108.5(3) . . ?
F4 B2 N6 107.9(2) . . ?
F3 B2 N4 112.1(3) . . ?
F4 B2 N4 110.9(3) . . ?
N6 B2 N4 106.0(2) . . ?
O2 C1 N1 119.3(3) . . ?
O2 C1 C2 121.9(3) . . ?
N1 C1 C2 118.8(2) . . ?
C3 C2 C10 120.2(3) . . ?
C3 C2 C1 120.2(3) . . ?
C10 C2 C1 119.6(3) . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 123.2(3) . . ?
C5 C6 C10 118.7(3) . . ?
C7 C6 C10 118.1(3) . . ?
C8 C7 C6 121.2(3) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 120.9(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C11 C9 C8 120.2(3) . . ?
C11 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C2 C10 C11 120.4(3) . . ?
C2 C10 C6 119.6(3) . . ?
C11 C10 C6 120.0(3) . . ?
C9 C11 C10 119.6(3) . . ?
C9 C11 C12 120.8(3) . . ?
C10 C11 C12 119.6(2) . . ?
N2 C12 N1 123.4(3) . . ?
N2 C12 C11 116.5(2) . . ?
N1 C12 C11 120.1(3) . . ?
N3 C13 N2 126.5(3) . . ?
N3 C13 S1 114.2(2) . . ?
N2 C13 S1 119.3(2) . . ?
C18 C14 C15 121.3(3) . . ?
C18 C14 S1 128.0(2) . . ?
C15 C14 S1 110.8(2) . . ?
C16 C15 C14 120.1(3) . . ?
C16 C15 N3 127.4(3) . . ?
C14 C15 N3 112.5(3) . . ?
C15 C16 C17 118.9(3) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C16 C17 C19 120.6(3) . . ?
C16 C17 H17 119.7 . . ?
C19 C17 H17 119.7 . . ?
C19 C18 C14 118.7(3) . . ?
C19 C18 H18 120.7 . . ?
C14 C18 H18 120.7 . . ?
O1 C19 C18 114.7(3) . . ?
O1 C19 C17 124.8(3) . . ?
C18 C19 C17 120.5(3) . . ?
O1 C20 C21 105.8(3) . . ?
O1 C20 H20A 110.6 . . ?
C21 C20 H20A 110.6 . . ?
O1 C20 H20B 110.6 . . ?
C21 C20 H20B 110.6 . . ?
H20A C20 H20B 108.7 . . ?
C22 C21 C20 113.9(3) . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 C23 113.4(4) . . ?
C21 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C24 C23 C22 113.6(4) . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 C25 113.5(4) . . ?
C23 C24 H24A 108.9 . . ?
C25 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C24 C25 C26 112.7(4) . . ?
C24 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
C24 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C27 C26 C25 114.6(4) . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
C25 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C26 C27 H27A 109.6 . . ?
C26 C27 H27B 109.1 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.7 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 N4 119.4(3) . . ?
O3 C28 C29 121.8(3) . . ?
N4 C28 C29 118.8(2) . . ?
C30 C29 C38 120.3(3) . . ?
C30 C29 C28 120.2(3) . . ?
C38 C29 C28 119.5(3) . . ?
C29 C30 C31 120.3(3) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C32 C31 C30 120.6(3) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C33 120.5(3) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C34 122.7(3) . . ?
C32 C33 C38 118.8(3) . . ?
C34 C33 C38 118.5(3) . . ?
C35 C34 C33 120.7(3) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 121.0(3) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C37 C36 C35 120.0(3) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 119.6(3) . . ?
C36 C37 C39 121.0(3) . . ?
C38 C37 C39 119.5(2) . . ?
C37 C38 C29 120.4(3) . . ?
C37 C38 C33 120.2(3) . . ?
C29 C38 C33 119.4(3) . . ?
N5 C39 N4 123.8(3) . . ?
N5 C39 C37 116.5(2) . . ?
N4 C39 C37 119.7(3) . . ?
N6 C40 N5 126.3(3) . . ?
N6 C40 S2 113.6(2) . . ?
N5 C40 S2 120.0(2) . . ?
C42 C41 C46 122.2(3) . . ?
C42 C41 S2 110.8(2) . . ?
C46 C41 S2 127.0(3) . . ?
C43 C42 C41 120.0(3) . . ?
C43 C42 N6 127.5(3) . . ?
C41 C42 N6 112.5(3) . . ?
C44 C43 C42 118.2(3) . . ?
C44 C43 H43 120.9 . . ?
C42 C43 H43 120.9 . . ?
C43 C44 C45 121.8(3) . . ?
C43 C44 H44 119.1 . . ?
C45 C44 H44 119.1 . . ?
O4 C45 C46 124.1(3) . . ?
O4 C45 C44 115.6(3) . . ?
C46 C45 C44 120.4(3) . . ?
C45 C46 C41 117.4(3) . . ?
C45 C46 H46 121.3 . . ?
C41 C46 H46 121.3 . . ?
O4 C47 C48 109.2(5) . . ?
O4 C47 H47A 109.8 . . ?
C48 C47 H47A 109.8 . . ?
O4 C47 H47B 109.8 . . ?
C48 C47 H47B 109.8 . . ?
H47A C47 H47B 108.3 . . ?
C49 C48 C47 110.8(7) . . ?
C49 C48 H48A 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 108.1 . . ?
C48 C49 C50 104.9(7) . . ?
C48 C49 H49A 110.8 . . ?
C50 C49 H49A 110.8 . . ?
C48 C49 H49B 110.8 . . ?
C50 C49 H49B 110.8 . . ?
H49A C49 H49B 108.8 . . ?
C51 C50 C49 116.1(8) . . ?
C51 C50 H50A 108.3 . . ?
C49 C50 H50A 108.3 . . ?
C51 C50 H50B 108.3 . . ?
C49 C50 H50B 108.3 . . ?
H50A C50 H50B 107.4 . . ?
C50 C51 C52 123.9(9) . . ?
C50 C51 H51A 106.3 . . ?
C52 C51 H51A 106.3 . . ?
C50 C51 H51B 106.3 . . ?
C52 C51 H51B 106.3 . . ?
H51A C51 H51B 106.4 . . ?
C53 C52 C51 118.0(8) . . ?
C53 C52 H52A 107.8 . . ?
C51 C52 H52A 107.8 . . ?
C53 C52 H52B 107.8 . . ?
C51 C52 H52B 107.8 . . ?
H52A C52 H52B 107.1 . . ?
C52 C53 C54 117.8(7) . . ?
C52 C53 H53A 107.9 . . ?
C54 C53 H53A 107.9 . . ?
C52 C53 H53B 107.9 . . ?
C54 C53 H53B 107.9 . . ?
H53A C53 H53B 107.2 . . ?
C53 C54 H54A 109.1 . . ?
C53 C54 H54B 110.0 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.3 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C12 N1 C1 121.5(2) . . ?
C12 N1 B1 122.6(2) . . ?
C1 N1 B1 116.0(2) . . ?
C12 N2 C13 119.0(2) . . ?
C13 N3 C15 112.4(2) . . ?
C13 N3 B1 122.1(2) . . ?
C15 N3 B1 125.5(2) . . ?
C39 N4 C28 122.0(2) . . ?
C39 N4 B2 122.6(2) . . ?
C28 N4 B2 115.3(2) . . ?
C39 N5 C40 119.0(2) . . ?
C40 N6 C42 112.8(2) . . ?
C40 N6 B2 122.2(2) . . ?
C42 N6 B2 124.9(2) . . ?
C19 O1 C20 119.6(3) . . ?
C45 O4 C47 119.9(4) . . ?
C13 S1 C14 90.10(14) . . ?
C40 S2 C41 90.23(14) . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        68.16
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.060
